Compound [Co-3(BTC) (HBTC) (H2BTC) (C2H4O2)(3)] . 3(DMF) . 6(H3O) was synthesized under mild conditions and its crystal structure was determined by using single crystal X-ray diffraction. The crystal structure was solved by direct method and refined by full-matrix least-square method. The crystal is monoclinic and belongs to space group Cc with a = 2.645 3 ( 5) nm, b = 1.670 4 (3) nm, c = 1.821 6(4) nm, beta = 128.16(3)degrees, V = 6.329(2) nm(3), Z = 2, D-c = 20.200 Mg/m(3) M-r = 1 314.744, mu = 10.274 mm(-1), F(000) = 38 226, GOF = 0.99, R = 0.094 1, omegaR = 0.257 3.